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Purification method of battery-grade graphite fluoride

A technology of fluorinated graphite and purification method, applied in the direction of carbon fluoride, etc., can solve the problems of affecting the battery storage capacity, the influence of the reaction kettle, and the large environmental pollution of chlorine gas, so as to improve the cleaning effect, wide application range and simple operation. Effect

Inactive Publication Date: 2012-07-25
SHANGHAI SCI BIO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of using graphite as raw material to prepare fluorinated graphite, it may affect the reactor and introduce new impurity ions. Therefore, controlling the purity of graphite still cannot meet the requirements of battery-grade fluorinated graphite, and the product must be fluorinated. The graphite is purified again to meet the requirements of battery grade fluorinated graphite
For fluorinated graphite, it is difficult to remove the extremely fine impurities impregnated in the graphite by flotation method. The chlorine gas used in the chlorination roasting method is very polluting to the environment, and the method of strong acid and alkali and high temperature can easily change its C-F bond. The structure of the battery affects the storage capacity of the battery, and the fluorinated graphite obtained after these treatments is still difficult to meet the battery level requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put 100Kg of fluorinated graphite with a fluorine content of 55%-61% and a purity of 99.5% in a 400L reaction vessel equipped with a stirrer, inject 100L of diluted 15% hydrofluoric acid solution, stir evenly, and then place in an ultrasonic In the process, filter after ultrasonication for 50min, the filter cake is placed in a hot furnace at 200°C to remove water and residual hydrofluoric acid, the total weight of the product is 99.8Kg, the product is off-white, and the fluorine content is The impurity ions are Fe<100ppm, Cu<50ppm, Ni<50ppm, meeting the battery material requirements.

Embodiment 2

[0018] Put 100Kg of fluorinated graphite with a fluorine content of 55%-61% and a purity of 99.2% in a 400L reaction vessel equipped with a stirrer, inject 150L of diluted 15% hydrofluoric acid solution, stir evenly, and then place it in an ultrasonic In the process, filter after ultrasonication for 60min. The filter cake is placed in a hot furnace at 200°C to remove water and residual hydrofluoric acid. The total weight of the product is 100Kg. The ions are Fe<100ppm, Cu<50ppm, Ni<50ppm, meeting the battery material requirements.

Embodiment 3

[0020] Put 100Kg of fluorinated graphite with a fluorine content of 50%-55% and a purity of 99.0% in a 400L reaction vessel equipped with a stirrer, inject 100L of diluted 20% hydrofluoric acid solution, stir evenly, and then place it in an ultrasonic After ultrasonication for 30 minutes, filter and repeat the above cleaning steps twice. Finally, put the filter cake in a hot furnace at 200°C to remove water and residual hydrofluoric acid. The total weight of the product is 99.5Kg, and the fluorine content is 50 %-55%, the impurity ions are Fe<100ppm, Cu<50ppm, Ni<50ppm, meeting the battery material requirements.

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Abstract

The invention discloses a purification method of ultrasound assisted HF (hydrogen fluoride) washing battery-grade graphite fluoride. The method comprises the following concrete steps of: mixing common graphite fluoride and 20% hydrofluoric acid uniformly; cleaning for 30-60 minutes under ultrasound assistance, and dissolving impurities fully; and then leaching the system above, placing a filter cake in a heat furnace of 150-200 DEG C and drying, thereby obtaining graphite fluoride meeting the battery-grade requirement. The purification method of ultrasound assisted HF washing battery-grade graphite fluoride provided by the invention is not only simple and convenient in process, is low in cost, but also is wide in application range, and is favor of industrial production.

Description

【Technical field】 [0001] The invention relates to a purification method of fluorinated graphite, more specifically, adopts an ultrasonic-assisted HF washing method to remove trace metal ions such as iron, copper and nickel in the fluorinated graphite, so as to meet the requirements of the battery level. 【Background technique】 [0002] Graphite fluoride is a graphite interlayer compound synthesized by the direct reaction of carbon and fluorine. The interlayer is a fluorine atom, which belongs to the covalent bond type interlayer compound. High fluoride graphite has excellent thermal stability, is an electrical and thermal insulator, and is not corroded by strong acids and alkalis. At any temperature, its wear life is better than that of MoS 2 As an additive to lubricating wax, it can significantly increase the bearing load of components and reduce the surface temperature of lubricated components. [0003] Graphite fluoride and lithium metal and dissolved LiClO 4 or LiBF 4 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00C01B32/10
Inventor 杨先金张艳
Owner SHANGHAI SCI BIO PHARMA
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